Treatment of fibrous material



Patented Nov. 3, 1931 warren STATES LEON LILIENFELD, OF VIENNA, AUSTRIA TREATMENT OF FIBROUS MATERIAL No Drawing. Application filed September 19, 1929, Serial No. 383,828, and in Austria June 9, 1927.

Difliculties are associated with the use of viscose or cellulose solutions as an agent for dressing woven textile materials or sizing yarn, on account of the fact that the fabric or yarn which has been thus treated acquires a stiff, paper-like and cold feel, and moreover its extensibility is rather low. Fabrics which have been dressed by means of viscose have also the disadvantage that the cellulose regenerated from the viscose applied to the fabric frequently undergoes rupture when the material is stretched or pulled, owing to the difference between the coefiicients of extensibility of the fabric and the coating, the result being that the coating exhibits numerous minute, or more or less coarse cracks. Even in textile printing, particularly in pigment printing with viscose, these defects are apparent to an undesirable degree, and the viscose layers printed on the textile have a stiff feel, and in many cases become torn on being stretched, especially when they are not very thin.

This invention relates to a process for treating textile fibrous material (whether in the form of woven fabrics or of yarn by dressing, sizing, printing, weighting 0 the like, by means of cellulose in dissolved form (for example viscose or a solution of cellulose in cuprammonia) from which cellulose 3 can be regenerated or precipitated respectively, whereby the foregoing disadvantages are minimized or remedied.

The invention consists in the application of the discovery that the properties of the dressing, sizing, printed layers or the like, which consist of. or contain cellulose regenerated from soluble derivatives of cellulose, for example from viscose or precipitated from a cel- 4 lulose solution, for example in cuprammonia, which has been applied to the fibrous material are improved, especially in respect of feel and extensibility,'if the dressing, sizing or coating contains hollow spaces or bubbles dispersed throughout it, or throughout at least a part of it. These hollows or small bubbles may be produced by dressing, sizing, or otherwise treating the material with a solution of a soluble modification of cellulose, for example viscose or with a solution of cellulose, containing a quantity of a gas or of a substance capable of being caused to evolve a gas by a suitable treatment or containing both a gas and a substance capable of being caused to evolve a gas. Thus textile fabrics or yarns as which have been dressed, sized or otherwise treated by means of viscose or a cellulose solution in accordance with the invention have a soft feel, even when the quantity of the dressing or the like is considerable. The so dressing is much lighter, and more downy, and therefore resembles the natural fibre more closely than do the dressings produced in the usual manner from viscose or cellulose solution which is free from gas, or contains as but little gas. Fabrics or yarns treated in accordance with the invention have also a warm feel, and owing to the hollows in the dressing, sizing or the like, it ispossible to produce even with small proportions of viscose or cellulose solution a very full, rich dressing or sizing. Material treated in accordance wit-h the invention has a good capacity for extension, and fissures or cracks do not occur when the material is pulled or stretched.

The hollow spaces may contain the gas, for example air or carbon dioxide, or the gas may be removed, wholly or in part, from them, for example, by dissolution, or with the aid of an increased or reduced pressure. '80

In treating fibrous material in accordance with this invention a gas, for example air, hydrogen or nitrogen, may be emulsified in a solution of a soluble modification of cellulose, forexample in crude or purified 8 viscose or in a solution of cellulose, for example in cuprammonia, by known methods, such as by injection, blowing, beating, agitation or the like or the gas may be d1ssolved in the viscose or other solution with the aid of pressure.

Another method of operating consists in incorporating with the viscose or solution of cellulose a substance, for example an alkali carbonate, an alkali sulphide or an alkali sulphite, which is capable of evolving a gas during the treatment for decomposing the viscose or precipitating the cellulose with an agent suitable for the regeneration or precipitation of the viscose respectively. The 109 substance capable of evolving a gas must be present in sufiicient concentration or amount as to yield enough gas to at least form fine bubbles of free gas in the viscose or cellulose solution. The viscose or cellulose solution containing a gas, or a substance capable of yielding a gas, or both a gas and a substance capable of yielding a gas, is then applied to or incorporated with a fabric or yarn, by hand or by means of a suitable machine. In order to cause the viscose or cellulose solution to penetrate more deeply into the fibre, this operation may, if desired, be conducted under reduced pressure, or under a raised pressure. There may be added to the viscose or cellulose solution another coating or siz ing agent, for instance starch, dextrin, albumen or gelatine; a softening agent, for instance, glycerine, soap, Turkey-red oil, glucose, castor oil, or paraffin oil; a filling material, for instance, talc or china clay; a

- pigment, for instance, zinc White, soot, or

powdered mica; or a dyestufi', or any two or more of these substances.

The cellulose may be regenerated from the viscose or precipitated from the cellulose solution in any known manner, by a suitable precipitating bath, or by other means, for instance, by heating, steaming, or merely by allowing t e treated material to stand.

If it is desired to expel the gas, for example air, contained in the hollows in order to permit the walls of the hollows to collapse, the gas may be removed for example by boiling with water, or by treatment with water under pressure. If the gas contained in the spaces is carbon dioxide, it may be dissolved partly in the precipitating bath, and partly during the subsequent washing operation. V

The following examples illustrate some methods by which the invention may be carried into effect, the parts being by weight:

E mam-ple 1.Air is injected into a viscose, made in any desired manner from matured or non-matured alkali-cellulose containing about 5-7 per cent. of cellulose on analysis, so as to produce an emulsion. A cotton fabric is dressed in known manner in a backfilling machine with the emulsion so produced, and the dressed material is treated in the wet state or after drying, to cause reversion of the viscose to cellulose by any precipitating bath known in the viscose art, or by steaming, for example, for 3-15 minutes at 105115 C. The material is then washed, dried and finished in the usual manner. If desired the washed and dried fabr1c may be steamed, for example, for 3-15 minutes at 105-115 0.

Emample 2.The procedure is as in Example 1, but with the exception that tale is added to the viscose in quantity amounting to about1-3 parts for each part of cellulose as determined by analysis.

E wmmple 3.100 parts of sulphite-cellulose containin 9-10 per cent of moisture, or 100 parts of lmters containing 7-8 per cent of moisture are impregnated at C. with 2000 parts of a solution of caustic soda of 18 per cent strength. After 3 hours, the soda cellulose is expressed until its total weight is 300 parts in the case of sulphite-cellulose or 340 parts in the case of linters, and coinminuted in a shredding machine for 2 5, to 3 hours. Before the soda cellulose has undergone any maturing, -60 parts of carbon-disulphide are added, and the mixture is allowed to react for 8 hours at 15l8 0.; at the end of this period any excess of carbondisulphidc which may be present is removed by blowing through a current of air for about 15 minutes, and the cellulose xanthate obtained is dissolved with the aid of a.

quantity of water, caustic soda and sodium carbonate, such that the solution produced contains about 1220 parts of water, about 107 parts of caustic soda and about 150 parts of sodium carbonate (reckoned as the anhydrous salt).

A suitable cotton fabric is dressed one or more times in a back-filling machine with the viscose produced in the manner just described, after it has been filtered or strained, and in the freshly prepared state, or after it has aged for 48-96 hours at 15 C. The dressed material is then immediately or after having been dried, introduced into sulphuric acid of 10 per cent strength or into any other acid precipitating bath known in the viscose industry, after which it is washed and dried. If desired, the dried fabric may be steamed, for example, for 315 minutes at 105-115 C. It will be understood that the material may be desulphurized or bleached in any known manner (for example by means of a solution of sodium sulphide) before or after it has been dried.

E wample l.-The procedure is as in Example 3, with'the exception that the alkali cellulose is allowed to stand for a period of 4:8- hours at room temperature before being treated with carbon disulphide.

- Ewample 5.-The procedure is as in Example 3 or Example 4, with the exception that talc is added to the viscose, for example, from 100 to 300 parts of the tale per 100 parts of cellulose.

Example 6.-The procedure is as in Example 1, Example 2, Example 3, Example 4, or Example 5, with the exception that there is added to the viscose about 1-2 per cent of its weight of paraflin oil or castor oil.

Example 7.-The procedure is as in any of the Examples 3-6, with the exception that the viscose has approximately the composition: 100 parts of parent cellulose, 1260 parts of water, 67 parts of caustic soda, and

150 parts of sodium carbonate (reckoned as the anhydrous salt).

3-8 contains about 6.5 to 6.7 per cent of cellulose which can be determined by analysis,

sodium carbonate being neglected. There:

may, however, be used a viscose containing a smaller proportion of cellulose, for example,

4-5 per cent.

Example 9.+-The procedure is as in any of the Examples 3-6, with the'difi'erence that the viscose has approximately the composition: 100 parts of parent cellulose, 1090 to 1130 parts of water, 240 to 200 parts of caustic soda and 125 to 100 parts of sodium carbonate (reckoned as anhydrous salt).

Eammple 10.l00 parts of a viscose containing sodium carbonate as used in anyof Examples 3-9 are intimately mixed with 5-8 parts of mica or with 10-15 parts of zinc white or 3 to 5 parts of soot. rial is then printed with this mixture in a Rouleaux machine. The further treatment and finishing are conducted in the manner described in the preceding examples.

In the preceding Examples 3-'-10, after having been coated or impregnated or printed, before washing, the fabric in the wet or dried state, may be steamed, for instance for 3-15 minutes at 105-115 C. and thereafter treated with the acid bath as in Example 3, washed and dried.

Examples for sizing yarn follow from the foregoing examples. 40

In carrying out the invention, instead of viscose, there may be used a solution of cellulose from which cellulose may be precipitated, for example a solution of cellulose in a thiocyanate solution such as calcium thiocyanate solution, a solution of cellulose in ammoniacal copper oxide solution, a solution of cellulose in an aqueous solution of a caustic alkali containing urea, thiourea or guanidine.

Fabrics and/or yarn dressed or sized respectively, with viscose or any cellulose solution, according to the present process, are

under the microscope different from fabrics or yarn filled or sized according to the processes known hitherto with viscose or cellulose solutions. The difference consists in the following: The small cellulose film particles that are on and between the fibres of the fabric or yarn, when produced after the present process, contain hollow spares and have consequently a spongy structure, whilst the small cellulose film particles formed on and between the fibres of fabrics and yarn that are filled with viscose or cellulose solutions according to the processes known heretofore, do not possess the spongy structure characteris- A cotton matetie of fabrics and yarn treated after the pres fabrics and yarn treated according to the present process.

It is to be understood that in the following -claims the term dressing the textile fibrous material includes any manner of application to the fibrous material, whether by manual or mechanical ,means and includes sizing, filling, impregnating, coating, weighting or printing a textile fibrous material, whether in the state of woven fabrics, or in the state of yarn.

The expression textile fibrous material in the specification and claims includes, wherever the context pcrmits, any spun or woven fibrous material, whether animal or Vegetable (for example, flax, linen, hem ramie, jute, wool and particularly cotton in the form of pure fabrics, or in the form of mixed fabrics,or in the form of yarn in skeins, cops or warps. I 1

The expression cellulose means in the description and claims: Cellulose and its near conversion products, such as cellulose hydrate, hydrocellulose and oxycellulose.

The present application is a continuation inpart of my copending application Serial Number 208,402 filed July 25, 1927, in which application I have claimed the product made by the processes described herein. In a copending case 305,875, filed September 13, 1928, I have claimed the process, as herein described, in which a substance capable of evolving a gas (e. g. sodium carbonate, sulfite or sulfide) is added to the viscose solution.

Having now particularly described my said invention and in what manner the same is to be performed, I claim:

1. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose, which solution contains a substance adapted to cause the formation ofhollows within at least a part of the cellulose, and thereafter treating the combination of textile fibrous material and solution to produce from the latter cellulose containing hollows.

2. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose, in which solution a gas is dispersed, and thereafter treating the combination of textile fibrous material and solution to pro- -which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and containing a gas emulsified in it, and thereafter treating the combination of textile'fibrous material and solution to produce cellulose from the latter.

4. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solutioncapable of yielding cellulose in which solution a gas is intimately mixed, and thereafter treating the combination of textile fibrous material and solution to produce cellulose from the latter.

5. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and a substance adapted to cause the formation of hollows within cellulose regenerated from the said viscose, and thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from theviscose.

6. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and in which a gas is dispersed, and thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose.

7'. A treatment of textile fibrous material which comprises dressing the textile fibrous material with-an agent comprising viscose and having a gas emulsified in it, and thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose.

8. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and in which a gas is intimately mixed, and thereafter treating the combination of textile fibrous material and agent to cause regenerationof cellulose from the viscose.

9. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and containing a substance adapted to cause the formation of gas containing hollows within at least a part of the yielded cellulose, thereafter treating the combination of textile fibrous material and solution to produce cellulose from the latter, and treating the combination of textile fibrous material and cellulose so obtained to remove gas at least in part from the hollows contained in the said combination.

10. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and in which a gas is dispersed throughout it for forming hollows within rial and cellulose so produced to remove gas at least in part from the hollows contained in the said combination.

12-. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and containing a gas intimately mixed in it, thereafter treating the combination of textile fibrous material and solution to produce cellulose from the latter, said gas being present in sufficient amount to form gas containing hollows in said cellulose and treating, the combination of textile fibrous material and cellulose so produced to remove gas at least in part from the hollows contained in the said combination.

13. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising. viscose and a substance adapted to cause the formation of gas containing hollows within cellulose regenerated from the said viscose, thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose and treating the combination of fibrous material and regenerated cellulose so produced to remove gas at least in part from the hollows contained in the said combination.

14. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and having a gas dispersed throughout it, thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose, said gas being present in suflicient amount to form gas containing hollows in said regenerated cellulose. and treating the combination of textile fibrous material and regenerated cellulose so produced to remove gas at least in part from the hollows contained in the said combination.

15. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and having a gas emulsified in it, thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose, said gas being present in sufficient amount to form gas containing hollows in said regenerated cellulose,

and treating the combination of textile fibrous material and regenerated cellulose so produced to remove gas at least in part from the hollows contained in the said combination.

16. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and having a gas intimately mixed in it, thereafter. treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose. said gas being present in sufiicient amount to form gas containing hollows in said regenerated cellulose, and treating the combination of textile fibrous material and regenerated cellulose so produced to remove gas at least in part from the hollows contained in the said combination.

17. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and containing a substance adapted to cause the formation of gas containing hollows within at least a part of the yielded cellulose, thereafter treating the combination of textile fibrous material and solution to produce cellulose from the latter, and treating the combination of textile fibrous material and cellulose so produced with a solvent for the gas contained in the hollows in the said combination to remove the said gas at least in part from the said hollows.

18., A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and containing a gas dispersed throughout it, thereafter treating the combination of textile fibrous material and-solution to produce cellulose from the latter, said gas being present in sufficient amount to form gas containing hollows in said cellulose, and treating the combination of textile fibrous material and cellulose so produced with a solvent for the said gas to remove gas at least in part from the hollows contained in the said combination.

19. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a. solution capable of yielding cellulose and containing a gas emulsified in it, thereafter treating the combination of textile fibrous material and solution to produce cellulose from the latter, said gas being present in sufiicient amount to form gas containing hollows in said cellulose, and treating the combination of textile fibrous mate rial and cellulose so produced with a solvent for the said gas to remove gas at least in part from the hollows contained in the said combination.

20. Atreatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose and which contains a gas intimately bination of textile fibrous material and solu-.

tion to produce cellulose from the latter, said gas being present in sutficient amount to form gas containing hollows in said cellulose, and treating the combination of textile fibrous material and cellulose so produced with a solvent for the said gas to remove gasat least in part from the hollows contained in the said combination.

21. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and a substance adapted to cause the formation of gas containing hollows within cellulose regenerated from the said viscose, thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose and treating the combination of textile fibrous material and regenerated cellulose so produced with a solvent for the gas contained in the hollows in the said combination, to remove gas at least in part from the said hollows.

22. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and a gas dispersed throughoutvit, thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose, said gas being present in sufiicient amount to form gas containing hollows in said cellulose and treating the. combination of textile fibrous material and regenerated cellulose so produced with a solvent for the said gas to remove gas at least in part from the hollows contained in the said combination.

23. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising viscose and having a gas emulsified in it, thereafter treating the combination of textile fibrous material and agent to cause regeneration of cellulose from the viscose, said gas being present in sufiicient amount to form gas containing hollows in said cellulose, and treating the combination of textile fibrous material and regenerated cellulose so produced with a solvent for the gas to remove gas at least in part from the hollows contained in the saidcombination.

24. A treatment of textile fibrous material which comprises dressing the textile fibrous material with an agent comprising v scose and a gas intimately mixed therein, thereafter treating the combination oftextile fibrous material and agent to cause regeneration of cellulose from the viscose, said gas being present in suflicient amount to form gas containing hollows in said cellulose, and treating the combination of textile fibrous material and regenerated cellulose so produced with a sol vent for the said gas to remove gas at least in part from the hollows contained in the said combination.

25. A treatment of textile fibrous material which comprises dressing the textile fibrous 5 material with a solution capable of yielding ccllulose,'which solution contains a substance adapted to cause the formation of numerous voids in the cellulose, and thereafter treating the combination of textile fibrous material 0 and solution to produce from the latter cellulose containing numerous voids, said substance being present in sufiicient amount that the cellulose from said solution has a spongy appearance under the microscope.

5 26. A treatment of textile fibrous material which comprises dressing the textile fibrous material with a solution capable of yielding cellulose, in which solution a gas is intimately mixed, and thereafter treating the combina- 0 tion of textile fibrous material and solution to produce cellulose from the latter, said gas being present in suflicient amount that the cellulose from said solution has a spongy appearance under the microscope.

5 In testimony whereof I affix my signature.

LEON LILIENFELD. 

